Ti doped NaAlH4 hydride is proposed as a reversible hydrogen storage material. In this work, the microstructure of NaAlH4 with 2% TiCl3 additive was studied after 5 hydrogen cycles using a combination of transmission electron microscopy (TEM) techniques including energy dispersive spectroscopy (EDS) X-ray analysis. Selected area diffraction and high-resolution (HR) imaging confirmed the presence of the NaH phase in the material. Electron diffraction was dominated by Al. HRTEM showed the presence of edge dislocations, which might influence the hydrogen diffusivity process in these materials.